CN1305540A - Process and apparatus for preparation of silicon crystals with preduced metal content - Google Patents
Process and apparatus for preparation of silicon crystals with preduced metal content Download PDFInfo
- Publication number
- CN1305540A CN1305540A CN99807420A CN99807420A CN1305540A CN 1305540 A CN1305540 A CN 1305540A CN 99807420 A CN99807420 A CN 99807420A CN 99807420 A CN99807420 A CN 99807420A CN 1305540 A CN1305540 A CN 1305540A
- Authority
- CN
- China
- Prior art keywords
- silicon
- protective layer
- crystal
- graphite
- equipment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/14—Heating of the melt or the crystallised materials
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10S117/90—Apparatus characterized by composition or treatment thereof, e.g. surface finish, surface coating
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1032—Seed pulling
- Y10T117/1068—Seed pulling including heating or cooling details [e.g., shield configuration]
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A method and apparatus for producing silicon single crystals with reduced contamination is disclosed. In one embodiment the structural components constructed of graphite and located in the hot zone of the crystal pulling apparatus have two protective layers. The first protective layer is applied directly to the graphite component. The second protective layer is a silicon layer and is applied on top of the first protective layer and covers the first layer. In a second embodiment, the structural components constructed of graphite and located in the hot zone of the crystal pulling apparatus have a single protective layer. The single protective layer is applied directly to the graphite and consists of a mixture of silicon carbide and silicon.
Description
The present invention relates to a kind of preparation method and equipment that reduces the single crystal silicon of pollutant load.More specifically, the present invention relates to a kind of preparation method and equipment of single crystal silicon, wherein, the Czochralski crystal lift structure graphite member in the crystal growing chamber of equipment coated two protective layers, comprise first protective layer, as silicon carbide or vitreous carbon and silicon second protective layer, perhaps apply a single protective layer that comprises silicon carbide and silicon mixture.
As the raw material of most of semiconductor element manufacturing processedes, silicon single crystal is used the preparation of so-called crystal pulling method (Czochralski) method usually.In this method, in polycrystalline silicon (" the polysilicon ") crucible of packing into, melt described polysilicon, seed crystal is immersed in the fused silicon, make silicon single crystal ingot long by lifting slowly to the diameter that requires.
The normally used crystal equipment of lifting is included in crucible many internal parts on every side that molten silicon is housed in crystal pulling method.These internal parts are with the graphite formation and be commonly referred to as " hot-zone " parts.These hot-zone parts, as pedestal, heating element, thermoshield, heat-reflecting body or lagging material, the hot-fluid around the control crucible and the speed of cooling of growing crystal.For a period of time, in this field, have realized that, though lifting graphite member used in the equipment at crystal does not directly contact with the crystal of molten silicon or growth, under the essential high temperature of the crystal of fusion polysilicon and growth gained, use these parts may cause the particulate venting, produce the melt of high-content pollutent, therefore produce the growing crystal that contains molybdenum, iron, copper, nickel, reaches other undesirable pollutent.As everyone knows, metals such as iron and molybdenum reduce the minority carrier lifetime in the silicon wafer, and copper and mickel can cause the oxygen in the gained crystal to induce stacking fault.Simultaneously, in crystal growing process, the oxygen that the interaction by silicon melt and crucible produces is present near the graphite member, may cause graphite oxidation, causes particle further to be emitted from the pore of graphite, and the reduction graphite-structure, causes part distortion.
In order to reduce, usually all graphite members in the hot-zone are applied protective barrier, as silicon carbide or vitreous carbon coating owing to being positioned at the contaminants crystalline danger that growing crystal graphite member venting on every side produces.Because its high-temperature oxidation resistance, silicon carbide is widely used in and is coated in crystal and lifts the graphite member that uses in the equipment hot-zone.Coat of silicon carbide provides a blocking layer that impurity is emitted by the sealing graphite surface, therefore requires impurity to pass through coating by crystal boundary and volume diffusion mechanism.Use this coating to be contained in crystal and lift the undesirable pollutent that produces by graphite in the process.The generally about 75-150 micron thickness of silicon carbide layer, and cover graphite surface.Scheiffarth and Wagner have described a kind of method of depositing silicon carbide layer on graphite at Surface and Coatings Technology (surface and coating technology) in 54/55 (1992) the 13-18 page or leaf.
Be similar to coat of silicon carbide, use the vitreous carbon coating to be contained in and be exposed to undesirable pollutent that graphite produces in the pyroprocess.People such as Lewis are in U.S. Patent No. 5,476, have described the method that the vitreous carbon coating is provided in 679 on graphite body.
Though on graphite, use coat of silicon carbide or vitreous carbon coating to reduce the amount of not wishing pollutent that enters in silicon melt and/or the growing crystal, but these two kinds of methods are being eliminated the particle contamination problems that is produced by graphite fully and are therefore all being got nowhere aspect the pollution of growing crystal.Even use silicon carbide or vitreous carbon coating, remain subject matter from the iron pollution of graphite.As if undesirable metal (as iron) can penetrate these coatings with the amount that is enough to reduce the gained crystal mass.Simultaneously, think that also typical silicon carbide coating itself that industry provides is by the iron pollution of about 1ppma.When this coating heated in the silicon crystal growing environment, iron may be diffused into the surface, evaporation, and be attached on the crystal of growth.
So, in semi-conductor industry, still need further to reduce the amount of pollutant that in crystal growing process, enters silicon melt owing to the particle that lifts the inner part generation of equipment hot-zone at crystal.
So, in purpose of the present invention, comprise a kind of method for preparing the silicon single crystal that reduces pollutant load that provides; Provide a kind of with the silicon carbide that applies on the silicon layer coated graphite parts or the method for vitreous carbon; A kind of method with silicon and silicon carbide mixture coated graphite parts is provided; A kind of method that absorbed the pollutent that causes the silicon crystal defective before it enters melt or crystal is provided; A kind of equipment that lifts that reduces the silicon single-crystal of metal pollutant content is provided; A kind of graphite member that can reduce by two protective layers of total metal pollutant content in the growing crystal that has is provided; A kind of graphite member that can reduce the single protective layer of total metal pollutant content in the growing crystal that has is provided; The method that increases total silicon single crystal output is provided.
So, in brief, the present invention relates to a kind of equipment that has the silicon single crystal that reduces metal pollutant content with the growth of Czochralski method.Described equipment comprises the growth room of a structure unit that quartz crucible is arranged and wherein arrange.Described structure unit is made of graphite, and applies with two different protective layers.Directly being coated on the graphite at lip-deep first protective layer of graphite-structure, can be silicon carbide or vitreous carbon.Second protective layer covers the first layer, and is made up of silicon.
The invention still further relates to a kind of equipment that has the silicon single crystal that reduces metal pollutant content with the growth of Czochralski method.Described equipment comprises the growth room of a structure unit that quartz crucible is arranged and wherein arrange.Described structure unit is made of graphite, and scribbles a protective layer, and described protective layer is made of the mixture of silicon carbide and silicon.
The invention still further relates to a kind of method that has the silicon single crystal of reduction metal pollutant content with the growth of Czochralski method.Described method be included in start before the crystal growing process with two independently protective layer apply by graphite and constitute and be arranged in structural part in the growth room.First protective layer on graphite surface is made of silicon carbide or vitreous carbon.Second coating is made of silicon and covers on first coating.After coating silicon coating on described parts, start crystal and lift process.
The invention still further relates to a kind of method that has the silicon single crystal of reduction metal pollutant content with the growth of Czochralski method.Described method applies the structural part that is made of graphite with a protective layer that is made of silicon carbide and silicon before being included in and starting crystal growing process.After the described protective layer of coating, start crystal and lift process.The invention still further relates to a kind of graphite member that two protective layers are arranged.First protective layer is made of silicon carbide or graphite carbon, and second protective layer is a silicon.
The invention still further relates to a kind of graphite member that a protective layer is arranged.Described protective layer is made of the mixture of silicon carbide and silicon.
Other purpose of the present invention and feature are will part clear, and part is pointed out hereinafter.
Fig. 1 is that silicon single crystal lifts equipment drawing.
Fig. 2 is the test-results figure of expression by iron pollution amount on the monitoring wafer of four various sample generations.
Fig. 3 is the Theoretical Calculation figure that is illustrated in the effect of silicon carbide on the graphite and silicon mixture protective coating.
Identical reference number is represented identical parts in all figure.
According to the present invention, have been found that the carborundum or the vitreous carbon that apply at graphite member apply Silicon protective coating, perhaps coating carbon on the graphite member of growth room that is positioned at crystal and lifts equipment The mixture protective coating of SiClx and silicon has obviously reduced the metal dirt that produces in grown crystal Dye thing. Advantageously, cover the carborundum be coated on the graphite or the silicon layer on the vitreous carbon, perhaps The silicon that mixes with carborundum, as under the required high temperature of grown crystal from graphite member or carborundum To the absorber of the pollutant (such as iron) of external diffusion, prevent from polluting metal and enter silicon melt in the coating Or the crystal of growth.
With reference now to figure,, particularly Fig. 1 has wherein represented generally to lift equipment at 2 crystal that represent. Described equipment comprises a crystal growing chamber 4 and crystal chamber 6. What comprise in crystal growing chamber is two Silica crucible 8 wherein contains the melting polycrystalline 26 that is useful on growing silicon single crystal. In operating process, Use is connected the crystal that lifts silk 10 slow pulling growths on the Winder. At crystal growing chamber Also comprise several structure members that consisted of by graphite in 4, be centered around around the described crucible, solid as being used for Decide crucible pedestal 14, heating silicon melt heater 16 and to be used for making heat remain on crucible attached Near heat shielding 18. As previously mentioned, these are arranged in the structure of crystal growing chamber " hot-zone " Parts are made of graphite, and the hot-fluid around the control crucible and the cooling velocity of silicon single crystal. Being familiar with should The technical staff in field should be realized that, other structural member that is made of graphite is such as reflector, gas Body purification pipe, observation panel passage or heat-barrier material also may be positioned at the hot-zone, and can basis Method preparation of the present invention.
The graphite that is used for structure hot-zone parts is generally the pure graphite at least about 99.9%, preferably extremely Few about 99.99% or purer graphite. Simultaneously, described graphite contains the total metal less than about 20ppm Content, such as iron, molybdenum, copper and nickel, preferably less than the total metal contents in soil of about 5ppm, as Iron, molybdenum, copper and nickel. In general, along with graphite purity improves, in high-temperature heating process The grain amount that produces reduces.
In one embodiment of the invention, said structure spare have the carborundum that covers described parts or Vitreous carbon first overcoat. The thickness of silication silicon or vitreous carbon first protective coating is generally about 75 Hes Between about 150 microns, preferably about 125 microns. Lift in the process at crystal, by the graphite structure The structural member that becomes and have carborundum or vitreous carbon coating is from Graphite Die Mold, Inc. (Durham, Conn.) buys. First overcoat is exposed in the pyroprocess as sealing and being contained in Barrier layer from graphite diffusion and the pollutant that discharges. Be used for crystal of the present invention and lift equipment Structural member an independently silicon second layer that covers on first overcoat is arranged.
Silicon overcoat on carborundum or vitreous carbon provides a protection against chemical as absorber to stop Layer, absorption can by the pollutant that produces from graphite of first overcoat, perhaps be prevented from first The pollutant that evaporates in the sheath is such as iron. Because silicon is to the high-affinity of pollutant, in the second layer Silicon easily and pollutant reaction, form stable silicide, such as Fe3Si, FeSi and FeSi2 Between pollutant and silicon layer, form stable silicide and acutely reduced the expansion of pollutant by silicon layer The ability of loosing. Therefore, realized that the pollutant that enters in silicon melt and the grown crystal obviously reduces.
By chemical vapour deposition technique known in this field, such as the high vacuum chemical vapour deposition (UHVCVD) or atmospheric pressure chemical vapour deposition (APCVD), the stone before using crystal growing process Growth protection silicon layer on the carborundum that applies on the China ink parts or the vitreous carbon. Be used for the protection silicon-containing layer deposition Suitable source gas comprises the gases such as a chlorosilane, dichlorosilane and trichlorosilane. These gases can To mix with the ratio of silane source with (for example) carrier gas of 30: 1 with carrier gas (such as hydrogen), with short Advance the growth of silicon layer.
Described silicon layer grows into thickness between about 0.1-3 micron, more at carborundum or vitreous carbon Preferably between about 0.5-2 micron, most preferably about 1 micron. Described protection silicon layer Can grow at the carborundum or the vitreous carbon that apply at graphite of one or more parts, to help In the crystal of growing, reduce the pollutant of gained. Yet, the described silicon layer of preferably growing, So that it covers following carborundum or the vitreous carbon that applies at graphite fully. If described silicon layer Layer below covering fully, the maximum protection that the crystal that can obtain that graphite granule is produced pollutes.
Can be under any temperature of the siliceous deposits that promotes to be undertaken by chemical vapour deposition the described silicon layer of growth.Suitable temperature range example is included between about 900 ℃-1300 ℃.Yet, to be familiar with the person skilled in art and to will recognize that, other temperature may be suitable, and may influence the sedimentation velocity of silicon on the graphite of coating silicon carbide.
In using the embodiment preferred of first and second protective layer, before being used for crystal growth equipment and process, by graphite constitute and structural part with silicon carbide or vitreous carbon coating through at least two independent siliceous depositss circulations, so that apply silicon carbide or vitreous carbon with the silicon that can fully absorb.The silicon of first deposition cycle about 0.1-1.5 micron of deposition on the surface of coating silicon carbide or vitreous carbon.Subsequently, rotating described structural part makes all parts of described parts all handle in the same manner with siliceous deposits.After rotation, beginning deposition cycle subsequently, the silicon of another about 0.1-1.5 micron of deposition on described surface.The structural part of gained has the silicon layer of an about 0.1-3 micron of thickness.After coating protection silicon layer, described parts can be used for crystal growing chamber and process, can pull out crystal from fused silicon liquid.
The structural part with two protective layers that is made of graphite of the present invention can be used for crystal of the present invention and lift equipment, and several the silicon single crystal of growing before described protection silicon layer is removed and replaces it.Preferably, utilize described parts growth 25-125 piece single crystal silicon, more preferably 100 blocks of silicon single crystal of growth before described protection silicon layer is removed or replaces it.Described protection silicon layer can remove with dilute acid soln (as diluted hydrofluoric acid).Described diluted acid is peeled silicon layer off, and former state stays the first following protective layer.Then, described graphite member can pass through above-mentioned chemistry of silicones vapour deposition, forms the second new protective layer on silicon carbide or vitreous carbon first protective layer.
In an alternate embodiment of the present invention, said structure spare has a single protective coating that directly is coated on the graphite surface.This single protective coating is made of the mixture of silicon carbide and silicon.Be similar to the above-mentioned embodiment of using two protective layers, with silicon carbide blended silicon as the cartridge that absorbs the pollutent that discharges from graphite member or silicon carbide itself and form stable silicide.
Described single protective layer is directly grown on aforesaid graphite member.The about 75-150 micron of the thickness of described single protective layer, comprises the silicon carbide of about 99.9-99.99% and the silicon of about 0.01-0.1%, preferably about 99.9% silicon carbide and about 0.1% silicon by preferably about 125 microns.
By the following example explanation the present invention, these embodiment only are used for explanation, and do not think and limit the scope of the invention or the mode of its enforcement.
In the present embodiment, handle graphite sample, on first protective layer, be formed for silicon second protective layer of embodiment 2 with silicon carbide first protective layer.
In the about 1100 ℃ tube furnace of temperature, the graphite sample of silicon carbide first protective layer with about 100 micron thickness is through the deposition cycle of two orders, protective layer of growth on silicon carbide layer.In each, the source gas of deposition protection silicon coating is to have 1: 30 the trichlorosilane and the mixture of hydrogen ratio at these two round-robin.Each circulation continues about 10 minutes, the about 1 micron silicon of deposition on silicon carbide.Described pressure is normal atmosphere.After first deposition cycle, rotate described sample, to guarantee fully to cover coat of silicon carbide with silicon.The sample of gained is made of the graphite of silicon second protective layer with silicon carbide first protective layer and about 2 micron thickness.
In the present embodiment, measure the graphite of the graphite be exposed to exposed graphite, coating vitreous carbon, coating silicon carbide and have silicon carbide first protective layer and the graphite of silicon second protective layer in the iron contaminants content of monitoring wafer.
The usage level boiler tube is exposed to four different samples to monitoring wafer by gaseous diffusion: 1) without any the graphite of protective coating; 2) graphite of 100 microns vitreous carbons of coating; 3) graphite of 100 microns silicon carbide of coating; 4) have silicon carbide first protective layer of about 100 micron thickness and silicon second protective layer of about 2 micron thickness.Use fumed silica dividing plate separating monitoring wafer and each sample, and prevent the direct contact between monitoring wafer and sample.Several holes on dividing plate make monitoring wafer can be exposed to the gas that produces from sample material.Each test group by be used for measuring by diffusion transmit the iron amount monitoring wafer, form at fumed silica dividing plate on the monitoring wafer and the sample on the hole at dividing plate.For each test, use wafer sample as a setting, there are not dividing plate or sample thereon.
Each of four samples of test is three differing tempss: 800 ℃, 950 ℃ and 1100 ℃, measure the iron diffusivity from the sample to the monitoring wafer.Described sample is kept under atmospheric pressure carrying out 2 hours thermal treatment, and remain on the described wafer and pass through argon gas stream.
After each thermal treatment, use the minority carrier lifetime (the iron amount of existence) of testing each monitoring wafer of each sample in the photoelectric technology described in the ASTM Report F391-78.On each sample, test the concentration of iron of some, and be recorded in the mean value of concentration of iron on the described wafer.Data based heat treatment time of the concentration of iron of 12 sample gained and wafer thickness are separated, and the curve of on logarithmic coordinates, draw every square centimeter of atomicity hourly and absolute temperature (1/ ℃+273).The result is shown in Fig. 2.
As shown in Figure 2, has the graphite sample of silicon carbide first protective coating and silicon second protective coating, the iron amount minimum that spreads on from the sample to the monitoring wafer.As shown in Figure 2, too low for the iron amount that on the monitoring wafer of 800 ℃ graphite sample, exists with silicon carbide first protective layer and silicon second protective layer, can not detect by described analytical procedure, so, for this sample, there is not the determination data point at 800 ℃.In all three temperature,, realized the remarkable reduction of iron diffusivity by using silicon second protective layer on the graphite sample of coating silicon carbide.
Embodiment 3
In the present embodiment, utilize epuilibrium thermodynamics to calculate, calculated under argon atmospher, the iron amount of from the mixture of the silicon that contains silicon carbide, various content and iron, evaporating.
Described calculation assumption, argon gas are 0.016mbar, and used temperature range is 600-1400 ℃.Every kind of mixture is by 0.1 mole of silicon carbide and 1 * 10
-7The iron of mole is formed.This ratio is equivalent to 100cm
2Silicon carbide, 125 micron thickness contain the iron of 1ppma.
The silicon amount that is incorporated in the silicon carbide changes to 1000ppma from the 0ppma of described silicon carbide-iron mixture.Use 1 mole argon gas to set up the volume of thermodynamic system.Fig. 3 represents from 1 * 10
-7The free iron of mole and excess silicon and have 10,100 and the calculating mole number of the iron steam of the silicon carbide-iron mixture gained of 1000ppma silicon never.
Fig. 3 shows, by increasing and coat of silicon carbide blended silicon amount, has obviously reduced the release of the coat of silicon carbide of iron steam contamination.As shown in the figure, calculate the mixture of 1000ppma silicon in silicon carbide, reduce iron steam discharging amount to about 1/100 by this coating, be reduced to about 1/1000 at 700 ℃ at 1200 ℃.
(second edition software carries out the calculating that iron discharges from silicon carbide-silicon-iron mixture for Pori, Finland) the HSC Chemistry of exploitation publication to use Outkumpu Research.
For above-mentioned reasons, as can be seen, can obtain several purpose of the present invention.
Owing in aforesaid method or equipment, can carry out various variations, and do not leave scope of the present invention, so it is illustrative to mean that all the elements that comprised in the above-mentioned specification sheets should be interpreted as, and meaning without limits.
Claims (10)
1. a crystal that has the silicon single crystal that reduces metal pollutant content by Czochralski grown lifts equipment, and described equipment comprises:
A growth room; With
Be arranged in the structural part in the growth room, described parts comprise graphite and have first protective layer of covering graphite and second protective layer on first protective layer, and described second protective layer is silicon and covers on first protective layer.
2. according to the equipment of claim 1, wherein, the thickness of described second protective layer on described structural part is about the 0.1-3 micron.
3. a crystal that has the silicon single crystal that reduces metal pollutant content by Czochralski grown lifts equipment, and described equipment comprises:
A growth room; With
Be arranged in the structural part in the growth room, described parts comprise graphite and have a protective layer that covers graphite, and described protective layer comprises silicon and the about 99.9-99.99% silicon carbide of about 0.01-0.1%.
4. according to the equipment of claim 7, wherein, the thickness of described protective layer and is made up of about 0.1% silicon and about 99.9% silicon carbide between about 75-125 micron.
5. one kind is controlled at the method that lifts the metal pair silicon single crystal ingot pollution that used graphitiferous parts are followed in the equipment in the silicon crystal process of growth at crystal, and described method comprises:
Lift the structural part of the graphite formation of using in the growth room of equipment with second protective layer coating crystal of first protective layer that covers described parts and covering first protective layer; With
Lift silicon single-crystal the molten silicon liquid in described growth room.
6. according to the method for claim 9, wherein, the thickness of described second protective layer is between about 0.1-3 micron.
7. one kind is controlled at crystal in the silicon crystal process of growth and lifts the method that used graphitiferous parts are followed in the equipment metal pair silicon single crystal ingot pollutes, and described method comprises:
Apply the structural part that crystal lifts the graphite formation of using in the growth room of equipment with the protective layer that covers described parts, described protective layer comprises silicon and the about 99.9-99.99% silicon carbide of about 0.01-0.1%; With
Lift silicon single-crystal the molten silicon liquid in described growth room.
8. according to the method for claim 15, wherein, about 125 microns of the thickness of described protective layer, and form by about 99.9% silicon carbide and about 0.1% silicon.
9. parts that are used for silicon single-crystal pullup equipment, described parts comprise graphite and have first protective layer that covers described graphite and second protective layer that covers described first protective layer, and wherein, described second protective layer is a silicon.
10. one kind is used for the parts that silicon single crystal lifts equipment, and described parts comprise graphite and have a protective layer, and described protective layer comprises the silicon of about 0.01-0.1% and the silicon carbide of about 99.9-99.99%.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US09/097,779 US6183553B1 (en) | 1998-06-15 | 1998-06-15 | Process and apparatus for preparation of silicon crystals with reduced metal content |
| US09/097,779 | 1998-06-15 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1305540A true CN1305540A (en) | 2001-07-25 |
| CN1220799C CN1220799C (en) | 2005-09-28 |
Family
ID=22265089
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB998074209A Expired - Fee Related CN1220799C (en) | 1998-06-15 | 1999-06-14 | Process and apparatus for preparation of silicon crystals with preduced metal content |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US6183553B1 (en) |
| EP (1) | EP1090167B1 (en) |
| JP (1) | JP4683725B2 (en) |
| KR (1) | KR100622331B1 (en) |
| CN (1) | CN1220799C (en) |
| DE (1) | DE69901183T2 (en) |
| TW (1) | TWI251038B (en) |
| WO (1) | WO1999066108A1 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020144642A1 (en) * | 2000-12-26 | 2002-10-10 | Hariprasad Sreedharamurthy | Apparatus and process for the preparation of low-iron single crystal silicon substantially free of agglomerated intrinsic point defects |
| KR20020096097A (en) * | 2001-06-16 | 2002-12-31 | 주식회사 실트론 | A Growing Apparatus of a single crystal ingot |
| US20070074653A1 (en) * | 2005-09-30 | 2007-04-05 | Memc Electronic Materials, Inc. | Apparatus for preparation of silicon crystals with reduced metal content |
| SG188933A1 (en) * | 2008-12-30 | 2013-04-30 | Memc Singapore Pte Ltd | Methods and pulling assemblies for pulling a multicrystalline silicon ingot from a silicon melt |
| JP5477229B2 (en) | 2010-08-26 | 2014-04-23 | 信越半導体株式会社 | Semiconductor single crystal manufacturing apparatus and manufacturing method |
Family Cites Families (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL244520A (en) | 1958-10-23 | |||
| DE2739258C2 (en) | 1977-08-31 | 1985-06-20 | Wacker-Chemitronic Gesellschaft für Elektronik-Grundstoffe mbH, 8263 Burghausen | Process for applying a protective layer containing silicon carbide and silicon nitride to shaped carbon bodies |
| US4288495A (en) | 1978-05-19 | 1981-09-08 | Ford Motor Company | Article coated with beta silicon carbide and silicon |
| US4621017A (en) | 1982-04-15 | 1986-11-04 | Kennecott Corporation | Corrosion and wear resistant graphite material and method of manufacture |
| US4617232A (en) | 1982-04-15 | 1986-10-14 | Kennecott Corporation | Corrosion and wear resistant graphite material |
| US4911896A (en) * | 1986-07-24 | 1990-03-27 | General Electric Company | Fused quartz member for use in semiconductor manufacture |
| JPS63166789A (en) * | 1986-12-26 | 1988-07-09 | Ibiden Co Ltd | Graphite crucible used in pulling up device for silicon single crystal and production thereof |
| DE3743951A1 (en) * | 1986-12-26 | 1988-07-07 | Toshiba Ceramics Co | Apparatus for pulling silicon single crystals containing a heat-insulating cylinder, and method for preparing the material of the latter |
| JPH0218375A (en) | 1988-07-07 | 1990-01-22 | Toshiba Ceramics Co Ltd | Device for pulling up semiconductor single crystal |
| US5041308A (en) | 1988-12-21 | 1991-08-20 | Osaka Titanium Co., Ltd. | Method of coating silicon particles |
| KR930004506A (en) | 1991-08-29 | 1993-03-22 | 티모티 엔. 비숍 | Glassy Carbon Coated Graphite Components Used to Grow Silicon Crystals |
| US5358603A (en) | 1992-10-06 | 1994-10-25 | Albemarle Corporation | Process for the removal of a silicon coating from a surface |
| JPH06127925A (en) | 1992-10-16 | 1994-05-10 | Tonen Chem Corp | Heat resistant cylindrical body, reaction tube for production of polycrystalline silicon and its production |
| US5405658A (en) | 1992-10-20 | 1995-04-11 | Albemarle Corporation | Silicon coating process |
| JPH0789789A (en) * | 1993-09-20 | 1995-04-04 | Fujitsu Ltd | Si crystal, method for growing crystal and device therefor |
| US5417803A (en) | 1993-09-29 | 1995-05-23 | Intel Corporation | Method for making Si/SiC composite material |
| JP2741164B2 (en) | 1994-03-16 | 1998-04-15 | 住友シチックス株式会社 | Graphite member for semiconductor single crystal pulling device and semiconductor single crystal pulling device |
| JPH10139581A (en) * | 1996-09-10 | 1998-05-26 | Toyo Tanso Kk | High-temperature member for device for pulling up single crystal |
-
1998
- 1998-06-15 US US09/097,779 patent/US6183553B1/en not_active Expired - Lifetime
-
1999
- 1999-06-14 WO PCT/US1999/013378 patent/WO1999066108A1/en active IP Right Grant
- 1999-06-14 DE DE69901183T patent/DE69901183T2/en not_active Expired - Lifetime
- 1999-06-14 EP EP99927525A patent/EP1090167B1/en not_active Expired - Lifetime
- 1999-06-14 CN CNB998074209A patent/CN1220799C/en not_active Expired - Fee Related
- 1999-06-14 JP JP2000554909A patent/JP4683725B2/en not_active Expired - Fee Related
- 1999-06-14 KR KR1020007014047A patent/KR100622331B1/en not_active IP Right Cessation
- 1999-07-23 TW TW088109999A patent/TWI251038B/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| EP1090167B1 (en) | 2002-04-03 |
| CN1220799C (en) | 2005-09-28 |
| KR100622331B1 (en) | 2006-09-13 |
| TWI251038B (en) | 2006-03-11 |
| DE69901183D1 (en) | 2002-05-08 |
| EP1090167A1 (en) | 2001-04-11 |
| JP2002518286A (en) | 2002-06-25 |
| DE69901183T2 (en) | 2003-01-16 |
| KR20010052754A (en) | 2001-06-25 |
| US6183553B1 (en) | 2001-02-06 |
| WO1999066108A1 (en) | 1999-12-23 |
| JP4683725B2 (en) | 2011-05-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2854201B2 (en) | Vitreous carbon-coated graphite part used for silicon crystal production and method for producing the same | |
| EP0308308B1 (en) | Apparatus for czochralski single crystal growing | |
| WO2004036657A1 (en) | Polycrystalline silicon substrate | |
| EP1178132A2 (en) | SiC material and method for manufacturing same | |
| US5882807A (en) | Jig for heat treatment and process for fabricating the jig | |
| CN1220799C (en) | Process and apparatus for preparation of silicon crystals with preduced metal content | |
| JPH062637B2 (en) | Single crystal pulling device | |
| KR102571434B1 (en) | Method of coating silica crucibles with silicon nitride | |
| US20020144647A1 (en) | Method of producing silicon carbide | |
| CN1208265C (en) | Apparatus and process for the preparation of low-iron contamination single crystal silicon | |
| JPH10144698A (en) | Silicon wafer and its manufacture | |
| WO2004000756A1 (en) | Method for forming semiconductor processing components | |
| RU2370568C1 (en) | Method of fabrication of quartz containers | |
| US20020071803A1 (en) | Method of producing silicon carbide power | |
| JPH0583517B2 (en) | ||
| JPH01290521A (en) | Jig for heat treatment | |
| JPS5950626B2 (en) | Container for pulling silicon single crystals | |
| Neugebauer et al. | Vertical Bridgman growth of large-diameter (Cd, Zn) Te crystals | |
| JPS6338541A (en) | Refining method for indium | |
| JPS6385075A (en) | Diffusion furnace process tube for semiconductor | |
| Hubbard | Zone refining high-purity germanium | |
| Khattak et al. | Processing of MG silicon for photovoltaic applications | |
| US20020071804A1 (en) | Method of producing silicon carbide: high temperature sensor elements | |
| JPH09235144A (en) | Material for semiconductor producing apparatus and production thereof | |
| Hubbard et al. | To be published in the Proceedings of the IEEE Nuclear Science Symposium, San Francisco, CA, October 19-21, 1977 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20050928 Termination date: 20140614 |
|
| EXPY | Termination of patent right or utility model |